Industrial method for clean recovery of olanzapine mother solution

A olanzapine parenteral and clean technology, applied in the direction of organic chemistry, can solve the problems of environmental pollution, waste of economic value of olanzapine, and no recycling of organic solvents, so as to reduce environmental pollution, reduce emissions, and extremely The effect of economic value and social value

Inactive Publication Date: 2020-04-07
PKU HEALTHCARE CORP LTD
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In the above-mentioned published literature, about 37.2% to 17.2% of olanzapine remains in the mother liquor in the refining step of the preparation route, ca

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Industrial method for clean recovery of olanzapine mother solution
  • Industrial method for clean recovery of olanzapine mother solution
  • Industrial method for clean recovery of olanzapine mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Referring to the preparation method of patent CN1179160A, add 20kg olanzapine crude product and 200L ethyl acetate into the reaction tank, heat up and dissolve, cool down and crystallize, and get about 200L olanzapine mother liquor after rejection filtration, and obtain 14.5kg olanzapine after drying the filter cake Flat, yield 72.5%;

[0041] Transfer the olanzapine mother liquor into the distillation tank, heat up and distill to recover the solvent ethyl acetate, stop the recovery when the solid precipitates in the tank, recover about 140L of ethyl acetate, the content is 99.3%, and the recovery rate is 70.0%, and then decompress and dry the tank inner material;

[0042] Add 60kg of water into the tank, start stirring, adjust the pH value to 3.0 with hydrochloric acid, heat up to 40°C to dissolve, and obtain a clear and transparent liquid through the ultrafiltration membrane module, transfer it to the crystallization tank, and oxidize it with 10% hydrogen The pH valu...

Embodiment 2

[0044] Referring to the preparation method of patent CN1466588A, add 20kg olanzapine crude product and 90L dichloromethane into the reaction tank, add activated carbon to decolorize after heating up and dissolving, crystallize after pressure filtration, obtain about 70L olanzapine mother liquor after rejection filtration, and dry the filter cake Afterwards, 12.5kg olanzapine was obtained, with a yield of 62.5%;

[0045] Transfer the olanzapine mother liquor into a distillation tank, heat up and distill to recover the solvent dichloromethane, stop the recovery when solids are precipitated in the tank, recover about 48L of dichloromethane, the content is 99.5%, and the recovery rate is 53.3%, and then decompress and dry the tank inner material;

[0046] Add 80kg of water into the tank, start stirring, adjust the pH value to 4.0 with acetic acid, heat up to 40°C to dissolve, and obtain a clear and transparent liquid through the ultrafiltration membrane module, transfer it to the ...

Embodiment 3

[0048] With reference to the preparation method of patent CN1420117A, 20kg olanzapine crude product and 200L ethanol were added into the reaction tank, after heating up and dissolving, activated carbon was added for decolorization, crystallization after pressure filtration, about 180L of olanzapine mother liquor was obtained after rejection filtration, and the filter cake was dried to obtain 15.9kg olanzapine, yield 79.5%;

[0049] Transfer the olanzapine mother liquor into the distillation tank, heat up and distill to recover the solvent ethanol, stop the recovery when solids are precipitated in the tank, recover about 152L of ethanol, with a content of 99.2%, and a recovery rate of 76.0%, and then decompress and dry the material in the tank;

[0050] Add 50kg of water into the tank, start stirring, adjust the pH value to 5.0 with acetic acid, heat up to 40°C to dissolve, and obtain a clear and transparent liquid through the ultrafiltration membrane module, transfer it to the ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides an industrial method for clean recovery of olanzapine mother solution. According to the method, on the basis of a production process in the prior art, a mother solution is distilled and concentrated to recycle a solvent, distillation residues are dissolved with water and acid, macromolecules and insoluble impurities are intercepted through an ultrafiltration membrane assembly, the pH value of the filtrate is adjusted with alkali, and the product olanzapine is separated out. The HPLC purity of the recovered olanzapine reaches 99.5% or above, and the recovered olanzapine can be directly refined to obtain qualified olanzapine. The clean and environment-friendly recycling and reusing process for the olanzapine mother solution solves the difficulty in recycling and reusing of the solvent and olanzapine in the mother solution, relieves heavy environmental protection burden for production enterprises, brings potential considerable economic benefits for manufacturers, and has high economic value and social value.

Description

technical field [0001] The invention belongs to the technical field of chemical medicines, and in particular relates to an industrial method for cleaning and recovering olanzapine mother liquor. Background technique [0002] Olanzapine is indicated for the treatment of schizophrenia and other psychosis with severe positive symptoms (e.g. delusions, hallucinations, disturbances in thinking, hostility and suspicion) and / or negative symptoms (e.g. apathy, emotional and social withdrawal, poor speech) Acute and maintenance therapy. Olanzapine also relieves secondary affective symptoms common in schizophrenia and related disorders. It has a therapeutic effect on mental disorders accompanied by Alzheimer's disease and Parkinson's disease. It was first listed in the United States in 1996 by Eli Lilly and Company of the United States. [0003] Its chemical name is 2-methyl-10-(4-methyl-1-piperazine)-4H-thieno[2,3-b][1,5]benzodiazepine. [0004] Its chemical structure is as shown...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D495/04
CPCC07D495/04
Inventor 邵波曾红孙玉娟袁平东吕勇均全继平
Owner PKU HEALTHCARE CORP LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap